CN103835003B - A kind of preparation method of bluish dogbane degummed ramie - Google Patents
A kind of preparation method of bluish dogbane degummed ramie Download PDFInfo
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- CN103835003B CN103835003B CN201310745959.3A CN201310745959A CN103835003B CN 103835003 B CN103835003 B CN 103835003B CN 201310745959 A CN201310745959 A CN 201310745959A CN 103835003 B CN103835003 B CN 103835003B
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Abstract
A preparation method for bluish dogbane degummed ramie, the Degumming method that the method utilizes vacuum technique and enzyme system and ultrasonic technology to combine comes unstuck to kenaf bast fiber.First utilize mixed enzyme system to come unstuck to bluish dogbane, utilize negative pressure of vacuum technology, make enzyme liquid fully to the inside entering fiber, make the large molecular breakdown of water-fast colloid, partial lignin is also decomposed simultaneously.Then utilize the ultrasonic wave of lower frequency to remove the colloid stronger with fibrous binding force, finally remove colloid remaining in the discreet portions such as micropore, gap with the ultrasonic wave of upper frequency.After this method solving single biological enzyme degumming, remaining colloid is many, the problems such as fiber surface is coarse, improves degummed ramie quality, decreases the use amount of enzyme and chemicals.
Description
Technical field
The present invention relates to crudefiber crop degumming technical field, be specifically related to a kind of preparation method of bluish dogbane degummed ramie.
Background technology
Bluish dogbane degummed ramie is by the flax fibre of bluish dogbane raw ramie after coming unstuck, and be the finished product of Degumming Procedures, its interior quality comprises the indexs such as fibrous fracture intensity, residual gum content, whiteness.
Containing multiple different chemical composition in bluish dogbane raw ramie, wherein content of cellulose is about 60%, and remaining non-cellulose components is colloid.The overwhelming majority in colloid is hemicellulose and lignin, and these colloids are enclosed in fiber appearance mostly, hemicellulose companion around cellulose, in network structure, pectin by the impurity such as hemicellulose and cellulose mutually cemented together.Therefore, in the process of refinement of bluish dogbane, coming unstuck is basis and crucial operation, and the quality of degumming effect directly has influence on the yield and quality of fiber, and then has influence on deep processing.
The method such as the method being applied to kenaf degumming now mainly contains that physics comes unstuck, chemical Degumming, biological degumming and materialization are come unstuck.The chemical Degumming method effect that textile industry generally uses is strong, but fibre damage is serious, and fiber strength declines comparatively large, and seriously polluted to environment; Although biological degumming technique is simple, energy consumption is low, few to the pollution of environment, there is not thorough, the ropy shortcoming of degummed ramie of coming unstuck.
In actual production, single Degumming method has a lot of deficiency, as not thorough, length consuming time etc. of coming unstuck of coming unstuck, finally also will be aided with additive method and come unstuck, just can reach the requirement of spinning quality.Therefore occurred the technique of a lot of combination degumming, as biochemical degumming, physical chemistry combination degumming method etc., the appearance of combined degum method, solves the problems such as crudefiber crop is come unstuck not thoroughly, quality of textile products is not up to standard, environmental pollution is serious.
Because bastose exists with the form of aggregate, adopt biological enzyme to come unstuck under normal conditions, the permeability only by biology enzyme self is difficult to enter into fibrous inside.Vacuum Freezing & Drying Technology is freezed by water-containing materials to form micro ice crystal under low-temperature condition, then under vacuum, micro ice crystal directly distilled the moisture sloughed in material, thus makes dry materials.In vacuum freeze drying, the structure of sample can not be destroyed, and so just remains the biological and chemical structure of material and the integrality of activity thereof, and can leave hole when ice distils.
It is under vacuum that vacuum enzyme comes unstuck, and by suction function and maceration, will be impregnated in bluish dogbane raw ramie fiber containing enzyme solutions, and make enzyme liquid fully enter into the inside of raw ramie, the contact area of enzyme liquid and colloid increases, and the degumming effect of enzyme liquid is strengthened greatly.In addition, because the cellulose commensal of bluish dogbane is more, glue-line is thick, sample must carry out the process such as washing decontamination, drying before Vaccum Permeating enzyme.
When high-strength ultrasonic is propagated in a liquid, huge energy can be discharged, can produce up to a hundreds of atmospheric local moment pressure, form shock wave, the surface of solids and liquid medium is made to be subject to great impulsive force and machinery " destruction " effect, its energy is enough to colloid and is separated with cellulose, so ultrasonic wave may be used for kenaf degumming.
The ultrasonic cavitation intensity of lower frequency is high, can remove and the colloid that numb adhesion is comparatively strong, particle is larger, but poor for the granule colloid effect in bluish dogbane micropore, gap; And the cavitation bubble that the ultrasonic wave of upper frequency produces can touch the granule colloid in micropore, itself and cellulose can be peeled off.Because the ultrasonic wave of upper frequency is very good to fiber micropore small particles colloid elimination effect, the bastose strength damage after process is little, cull is low, whiteness is higher.
The invention provides a kind of preparation method of novel bluish dogbane degummed ramie, utilize mixed enzyme system to come unstuck to bluish dogbane under vacuum, what then use lower frequency respectively removes remaining colloid with the ultrasonic wave of upper frequency.After this method solving single biological enzyme degumming, remaining colloid is many, the problems such as fiber surface is coarse, improves degummed ramie quality.
Summary of the invention
First object of the present invention is to provide a kind of preparation method of novel bluish dogbane degummed ramie, compare with physics Degumming method with traditional chemical Degumming, this Degumming method can obtain bluish dogbane bundle fiber best in quality, solve the problems such as fibre damage is large, environmental pollution is serious, and the brute force of fiber, feel, color and luster also etc. all meet the requirement of textile process.
Second object of the present invention is the problem such as to come unstuck thoroughly for current single Degumming method, fiber surface is coarse, fiber colour is poor, provides a kind of preparation technology's formula of novel bluish dogbane degummed ramie.The Degumming method utilizing vacuum technique and enzyme system and ultrasonic technology to combine comes unstuck to kenaf bast fiber, by test of many times Optimizing Process Parameters, and a kind of novel degumming tech formula of final formation.This technical recipe fully can remove the colloid of bluish dogbane, and make Degumming of Ramie greatly reduce, fiber surface is smooth, soft simultaneously, and color and luster is good, can meet the requirement of the aft-loaded airfoil such as textile printing and dyeing.
Implementation method of the present invention is as follows:
For realizing first object of the present invention, acted synergistically to kenaf degumming by vacuum technique and biology enzyme, the method utilizes Vacuum Freezing & Drying Technology make the colloid of bluish dogbane and cellulose initial gross separation and form a large amount of hole, then utilize negative pressure of vacuum dipping technique, dried bluish dogbane is placed in vacuum tank, first vacuumizes, then the enzyme solutions of low concentration is injected, make it fully be impregnated into bastose pore interior, the contact area of enzyme liquid and colloid is increased, thus play maximum effect.
For realizing second object of the present invention, the Degumming method adopting vacuum enzyme and ultrasonic wave to combine, utilizes mixed enzyme system to come unstuck to bluish dogbane first under vacuum, makes the large molecular breakdown of colloid, and partial lignin decomposes simultaneously.Then the ultrasonic wave of lower frequency is utilized to remove the colloid stronger with fibrous binding force, finally remove colloid remaining in the discreet portions such as micropore, gap with the ultrasonic wave of upper frequency, solve the problems such as remaining colloid is many, fiber surface is coarse, fiber colour is poor.
When bastose is for the production of high-grade fabric, higher to fiber performance requirements.Combine firm, that filament is shorter feature for bluish dogbane colloid, China does not but have corresponding standard to test above three indexs.Therefore, fibrous fracture intensity mainly measures on mono-fiber strong force instrument, the testing standard of residual gum content and whiteness reference ramie.
In the present invention based on the technological process of vacuum enzyme and ultrasonic technology and auxiliary process as follows:
Ultrasonic wave process → washing → dehydration → oil supply → washing → oven dry → the bastose of the ultrasonic wave process → upper frequency of bluish dogbane raw ramie → vacuum freeze drying process → vacuum ferment treatment → enzyme deactivation process → washing → lower frequency.
Process equipment: self-control multi-frequency supersonic generator, CHRIST type freeze drier (German MarinChrist company), DZF-6090 type vacuum laboratory box (Beijing permanent Tai Fengke testing equipment Co., Ltd), DZF-6020 constant temperature blast drying oven (Yuhua Instrument Co., Ltd., Gongyi City) etc.
The water that described bluish dogbane raw ramie is placed in about 20 DEG C soaks 2h, and take out and dry in the air to not dripping, then adjusting sample moisture content is 150%.
Described vacuum freeze drying process, is first placed in freeze drier through superfreeze post processing the bluish dogbane raw ramie regulating moisture content, and raw ramie internal water molecule forms micro ice crystal, the fracture of simultaneous part secondary bond; Then vacuumize under cryogenic, fibrous inside micro ice crystal directly distils in vacuum drying process, thus also forms many micropores at fiber surface and inside.Make fiber macromolecule internal structure become lax simultaneously, produce point fine a, filtration structures because the weak structure between filament or fibril is destroyed simultaneously.
The concrete operations technique of vacuum freeze drying process in this patent is: the moisture content bluish dogbane raw ramie that is 150% is placed in vacuum freeze drier and carries out freeze drying process: arrange minimum cryogenic temperature and be-60 DEG C, cooling time is 8h, then vacuum rewarming is carried out, vacuum is-0.1Mpa, and vacuum rewarming time is 60min.
Described vacuum ferment treatment utilizes vacuum technique that the enzyme preparation of low concentration is injected into fiber hole, and enzyme preparation is fully contacted with colloid, plays maximum effect.Hemicellulase, laccase etc. act on bastose, make the large molecular breakdown of colloid become Small molecular, and then are removed by glial component, make the kenaf bast fiber be bonded together be separated into available process of fiber.Put by enzyme degumming tech and carry out under vacuo, utilize negative pressure of vacuum technology, enzyme can be made to enter the inside of fiber, reaction is more abundant, and enzymatic activity improves, and reaction is accelerated.
In the present invention, vacuum enzyme treatment process is: moved on in vacuum laboratory box by the bluish dogbane after vacuum freeze drying process and carry out vacuum ferment treatment.Vacuumize and make vacuum in experimental box be-0.2Mpa, then inject the mixed solution of hemicellulase and laccase, and keep temperature to be 35 DEG C ~ 40 DEG C, processing time 24h.Wherein the concentration of hemicellulase and laccase is respectively 0.5%, 0.1%, and hemicellulase enzyme after dilution is lived as 80.00IU/ml, and laccase enzyme after dilution is lived as 150.00IU/ml, processing time 24h.
Described enzyme deactivation process carries out enzyme deactivation process to the bluish dogbane after vacuum ferment treatment, carries out enzyme deactivation process with high temperature washing or adjust ph.During described high temperature washing, the temperature of water is 80 DEG C ~ 100 DEG C; PH value when adjust ph carries out enzyme deactivation process is greater than 10.0 or be less than 4.0.
Dissolved matter on fiber, for adopting tap water bluish dogbane, is removed by described washing, rinse to PH be about 7.0 ~ 7.5.
The principle of described ultrasonic wave process is that high-strength ultrasonic is when propagating in a liquid, can energy-producingly intensify and happen suddenly, i.e. ultrasonic " cavitation effect ", it can discharge huge energy, can produce up to a hundreds of atmospheric local moment pressure, form shock wave, make the surface of solids and liquid medium be subject to great impulsive force and machinery " destruction " effect.The ultrasonic wave process intensity of lower frequency is high, the colloid stronger with numb adhesion can be removed, but cannot be deep into the discreet portions such as bluish dogbane micropore, gap, the shock wave penetration capacity that the ultrasonic wave process of upper frequency produces is strong, can remove the colloid that the discreet portions such as micropore, gap exists.
In the present invention the ultrasonic pretreatment of lower frequency be by bluish dogbane raw ramie with 1: 20 bath raio put into the solution that naoh concentration is 0.5%, be the ultrasonic wave process 2h of 4000W with 28KHz, power, each process bluish dogbane 5kg, maintains the temperature at about 50 DEG C.
In the present invention, the supersonic treatment of upper frequency is: the bluish dogbane after ferment treatment being placed on naoh concentration is carry out ultrasonic wave process in the solution of 0.5%, ultrasonic frequency is 56KHz, power is 6000W, at about 50 DEG C process 2h, each process bluish dogbane 5kg.
Described oil supply parameter is amino-modified silicone softener 4 ~ 6ml/L, temperature 35-45 DEG C, 25 ~ 30 minutes processing times, bath raio 1: 15 ~ 20.
Beneficial effect of the present invention is: (1) adopts mixed enzyme system to come unstuck to bluish dogbane under vacuum, and the degumming effect of enzyme liquid is strengthened greatly, and simultaneously used enzyme preparation concentration only has 5% of concentration under general case; (2) vacuum enzyme and ultrasonic wave synergistic reaction scouring processes very little to the damage ratio of fiber, fiber surface smooth pliable, color and luster is good, and spinnability improves greatly.
Detailed description of the invention:
A kind of preparation method of bluish dogbane degummed ramie, the Degumming method that the method utilizes vacuum technique and enzyme system and ultrasonic technology to combine comes unstuck to kenaf bast fiber, first mixed enzyme system is utilized under vacuum to come unstuck to bluish dogbane, utilize negative pressure of vacuum technology, make enzyme liquid fully to the inside entering fiber, can make the large molecular breakdown of water-fast colloid, partial lignin is also decomposed simultaneously, makes the kenaf bast fiber be bonded together be separated into available process of fiber.Then utilize the ultrasonic wave process removing of lower frequency and the stronger colloid of fibrous binding force, finally remove colloid remaining in the discreet portions such as micropore, gap with the ultrasonic wave process of upper frequency.
In the present invention based on the technological process of vacuum enzyme and ultrasonic technology and auxiliary process as follows:
Ultrasonic wave process → washing → dehydration → oil supply → washing → oven dry → the bastose of the ultrasonic wave process → upper frequency of bluish dogbane raw ramie → vacuum freeze drying process → vacuum ferment treatment → enzyme deactivation process → washing → lower frequency.
Above-mentioned degumming tech comprises the steps:
(1) water that the bluish dogbane raw ramie described in is placed in about 20 DEG C soaks 2h, and take out and dry in the air to not dripping, then adjusting sample moisture content is 150%.
(2) vacuum freeze drying process: the moisture content bluish dogbane raw ramie that is 150% is placed in vacuum freeze drier and carries out freeze drying process: minimum cryogenic temperature is set and is-60 DEG C, cooling time is 8h, then vacuum rewarming is carried out, vacuum is-0.1Mpa, and vacuum rewarming time is 60min.
(3) vacuum ferment treatment: the bluish dogbane after vacuum freeze drying process is moved on in vacuum laboratory box and carries out vacuum ferment treatment.Keep vacuum in experimental box to be-0.2Mpa, then inject the mixed solution of hemicellulase and laccase, and keep temperature to be 35 DEG C ~ 40 DEG C, processing time 24h.Wherein the concentration of hemicellulase and laccase is respectively 0.5%, 0.1%, and hemicellulase enzyme after dilution is lived as 80.00IU/ml, and laccase enzyme after dilution is lived as 150.00IU/ml, processing time 24h;
(4) enzyme deactivation process: carry out enzyme deactivation process with high temperature washing or adjust ph.During described high temperature washing, the temperature of water is 80 DEG C ~ 100 DEG C; PH value when adjust ph carries out enzyme deactivation process is greater than 10.0 or be less than 4.0;
(5) wash: adopt tap water bluish dogbane, enzyme is decomposed colloid produces dissolved matter remove.
(6) the ultrasonic wave process of lower frequency: by bluish dogbane raw ramie with 1: 20 bath raio put into the solution that naoh concentration is 0.5%, be the ultrasonic wave process 2h of 4000W with 28KHz, power, each process bluish dogbane 5kg, maintains the temperature at about 50 DEG C.
(7) the ultrasonic wave process of upper frequency: the bluish dogbane after ferment treatment being placed on naoh concentration is carry out ultrasonic wave process in the solution of 0.5%, ultrasonic frequency is 56KHz, power is 6000W, at about 50 DEG C process 2h, each process bluish dogbane 5kg.
(8) wash: adopt tap water bluish dogbane, the dissolved matter on fiber removed, rinse to PH be about 7.0 ~ 7.5;
(9) oil supply: amino-modified silicone softener 4 ~ 6ml/L, temperature 35-45 DEG C, 25 ~ 30 minutes processing times, bath raio 1: 15 ~ 20.
Vacuum technique is a ripe technology in electronic technology, food-dewatering etc., the present invention is innovatively attached to it in existing kenaf degumming technology and goes application, by being optimized combination to vacuum technique, biology enzyme, ultrasonic technology, make it to become a new application technology.And analyzed by great many of experiments, continue to optimize degumming tech parameter, finally obtain a kind of novel kenaf degumming technical recipe.This method solve after single Degumming method comes unstuck, remaining colloid is many, the problems such as fiber surface is coarse; And the alkali concn used is 0.5%, only come unstuck by general chemistry 1/10 of alkali consumption, greatly reduces fiber strength damage.By the mensuration to these three indexs of fibrous fracture intensity, residual gum content and whiteness, find that the powerful mean value of its fibrous fracture is 40cN ~ 50cN, residual gum content is down to about 3%, and fibre whiteness is up to about 80, and prepared degummed ramie quality is higher.
Claims (1)
1. the preparation method of a bluish dogbane degummed ramie, it is characterized in that utilizing vacuum technique and mixed enzyme system and ultrasonic technology to combine to the technique of bastose process is: first bluish dogbane raw ramie is placed in vacuum freeze drier and carries out freeze drying process, then bluish dogbane is moved on in vacuum laboratory box and carry out vacuum ferment treatment, wherein in vacuum laboratory box, vacuum is-0.2MPa, the mixed solution that the enzyme liquid used is hemicellulase and laccase, temperature is 35 DEG C ~ 40 DEG C, processing time 24h; Finally with frequency be 28KHz, power is ultrasonic wave removing and the stronger colloid of fibrous binding force of 4000W, then with frequency be 56KHz, power is the colloid that the ultrasonic wave of 6000W removes remnants in the discreet portions such as micropore, gap; Ultrasonic treatment time is 2h, and each process bluish dogbane is 5kg, and temperature is 50 DEG C.
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